Devices for use in solid-state NMR analysis

Abstract

The present disclosure relates to devices and methods for use in SSNMR analysis of solid particulate samples. These devices and methods are configured to contain a solid particulate sample as it undergoes SSNMR analysis while also operating to attenuate peak broadening in the resulting spectrum due to anisotropic dipole coupling interactions and CSA during such analysis by generating a substantially fluidized bed of the solid particulate sample.

What is claimed is: 
     
       1. A device for attenuating peak broadening during NMR analysis of a solid particulate sample comprising:
 (A) a sample container having an inner wall and sized to hold the solid particulate sample; 
 (B) a motor; 
 (C) a non-magnetic, electrically non-conductive drive shaft having a first end and a second end, wherein the motor is fixably attached to the first end of the non-magnetic, electrically non-conductive drive shaft; and 
 (D) a non-magnetic, electrically non-conductive impeller, wherein the non-magnetic, electrically non-conductive impeller is fixably attached to the second end of the non-magnetic, electrically non-conductive drive shaft and the non-magnetic impeller is located inside the sample container; wherein the motor is gas-driven. 
 
     
     
       2. A device for attenuating peak broadening during NMR analysis of a solid particulate sample comprising:
 (A) a sample container having an inner wall and sized to hold the solid particulate sample; 
 (B) a motor; 
 (C) a non-magnetic, electrically non-conductive drive shaft having a first end and a second end, wherein the motor is fixably attached to the first end of the non-magnetic, electrically non-conductive drive shaft; and 
 (D) a non-magnetic, electrically non-conductive impeller, wherein the non-magnetic, electrically non-conductive impeller is fixably attached to the second end of the non-magnetic, electrically non-conductive drive shaft and the non-magnetic impeller is located inside the sample container; wherein the motor is magnetic and/or electrically-driven and is shielded from the NMR magnet. 
 
     
     
       3. The device of  claim 2 , wherein the shielding is active. 
     
     
       4. The device of  claim 2 , wherein the shielding is passive. 
     
     
       5. The device of  claim 2 , wherein the non-magnetic, electrically non-conductive shaft comprises carbon-filled PEEK. 
     
     
       6. A device for attenuating peak broadening during NMR analysis of a solid particulate sample comprising:
 (A) a sample container sized to hold the solid particulate sample; 
 (B) a motor located at a distance from the sample container such that a magnetic field strength of a NMR magnet used to analyze the solid particulate sample in the sample container is about 0.5 millitesla or less at the distance; 
 (C) a first and a second non-magnetic, electrically non-conductive drive shaft, wherein each non-magnetic, electrically non-conductive drive shaft has a first end and a second end, wherein (1) the motor is fixably attached to the first end of the first non-magnetic, electrically non-conductive drive shaft and (2) the first end of the second non-magnetic, electrically non-conductive drive shaft is fixably attached to the second end of the first non-magnetic, electrically non-conductive drive shaft through a transmission gear box; and 
 (D) a non-magnetic, electrically non-conductive impeller fixably attached to the second end of the second non-magnetic, electrically non-conductive drive shaft, wherein the non-magnetic, electrically non-conductive impeller is located inside the sample container. 
 
     
     
       7. The device according to  claim 6 , wherein the transmission gear box comprises a 90 degree transmission gear box. 
     
     
       8. The device according to  claim 6 , wherein the motor drives the non-magnetic, electrically non-conductive impeller at a rate to generate a substantially fluidized bed of the solid particulate sample. 
     
     
       9. A device for attenuating peak broadening during NMR analysis of a solid particulate sample comprising:
 (A) a sample container sized to hold the solid particulate sample; 
 (B) a motor located at a distance from the sample container, the distance selected such that substantially no disruption is caused to NMR analysis of the solid particulate sample; 
 (C) a first and a second non-magnetic, electrically non-conductive drive shaft, wherein each non-magnetic, electrically non-conductive drive shaft has a first end and a second end, wherein (1) the motor is fixably attached to the first end of the first non-magnetic, electrically non-conductive drive shaft and (2) the first end of the second non-magnetic, electrically non-conductive drive shaft is fixably attached to the second end of the first non-magnetic, electrically non-conductive drive shaft through a transmission gear box; and 
 (D) a non-magnetic, electrically non-conductive impeller fixably attached to the second end of the second non-magnetic, electrically non-conductive drive shaft, wherein the non-magnetic, electrically non-conductive impeller is located inside the sample container.